反应详情

A mixture of 4'-fluoro-2'-chloroacetophenone (40 g), methylamine (33% w/w solution in industrial methylated spirit, 60 ml), industrial methylated spirit (40 ml) and copper powder (0.5 g) was stirred at 80° in a sealed pressure vessel for 3 hours. After cooling to ambient temperature, the reaction mixture was transferred to a conical flask. The reaction vessel was washed out with industrial methylated spirit (2×30 ml) and the washings added to the reaction mixture. Sodium sulphide nonahydrate (2.3 g) in water (23 ml) was added and the mixture heated at 50° for 10 minutes. The mixture was filtered through diatomaceous earth (sold under the trade name CELITE). Solvent was removed from the filtrate under reduced pressure at 40° and hydrochloric acid (5M, 160 ml) was added to the residue. The mixture was stirred for approximately 2 hours and then extracted with dichloromethane (100 ml, then 2×60 ml). The combined extracts were dried over magnesium sulphate and evaporated to give the novel compound 4'-fluoro-2'-(methylamino)acetophenone as an oil which solidified on storing at ambient temperature.

1. customthe reaction mixture was transferred to a conical flask
2. washThe reaction vessel was washed out with industrial methylated spirit (2×30 ml)
3. additionthe washings added to the reaction mixture
4. additionSodium sulphide nonahydrate (2.3 g) in water (23 ml) was added
5. temperaturethe mixture heated at 50° for 10 minutes
6. filtrationThe mixture was filtered through diatomaceous earth (
7. customSolvent was removed from the filtrate under reduced pressure at 40°
8. additionhydrochloric acid (5M, 160 ml) was added to the residue
9. stirringThe mixture was stirred for approximately 2 hours
10. extractionextracted with dichloromethane (100 ml
11. dry with materialThe combined extracts were dried over magnesium sulphate
12. customevaporated